Magnesium Hydroxide → 2-Hydroxyimino-2-(isothiazol-4-yl)acetic acid

HRID 1703019

Reaktionsgleichung

Reaktionsgleichung von HRID 1703019
[S:1]1[CH:5]=[C:4]([C:6](=O)[C:7]([OH:9])=[O:8])[CH:3]=[N:2]1.[OH-:11].[Mg+2].[OH-].Cl.[NH2:15]O>C(O)C.O>[OH:11][N:15]=[C:6]([C:4]1[CH:3]=[N:2][S:1][CH:5]=1)[C:7]([OH:9])=[O:8]

Komponenten

6

Edukt 3

HCID 73981Magnesium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 129065552-(Isothiazol-4-yl)glyoxylic acid

Produkt 1

HCID 571550852-Hydroxyimino-2-(isothiazol-4-yl)acetic acidAusbeute 76,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

A suspension of 2-(isothiazol-4-yl)glyoxylic acid (240 mg.), magnesium hydroxide (290 mg.) and hydroxylamine hydrochloride (140 mg.) in a mixture of ethanol (2 ml.) and water (10 ml.) was stirred for 2 hours at ambient temperature and allowed to stand overnight at ambient temperature. Ethanol was distilled off and to the residue was added ethyl acetate. The mixture was adjusted to pH 1 with 10% hydrochloric acid and the ethyl acetate layer was washed with water and dried over magnesium sulfate. The solvent was distilled off under reduced pressure to give 2-hydroxyimino-2-(isothiazol-4-yl)acetic acid (syn isomer) (0.20 g.), mp 159° to 161° C. (dec.).

Aufarbeitung

  1. waitto stand overnight at ambient temperature
  2. distillationEthanol was distilled off and to the residue
  3. additionwas added ethyl acetate
  4. washthe ethyl acetate layer was washed with water
  5. dry with materialdried over magnesium sulfate
  6. distillationThe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-c94da9d4f944490698e7bd0352b12546
Quelldatensatz
uspto-grants-1982_09
Patentnummer
US04350693

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